CN106634880B - Preparation method of amphiphilic starch fluid loss additive for water-based drilling fluid - Google Patents
Preparation method of amphiphilic starch fluid loss additive for water-based drilling fluid Download PDFInfo
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Abstract
The invention relates to a preparation method of an amphiphilic starch filtrate reducer for water-based drilling fluid, which is used in the drilling process of petroleum exploration wells and production wells. The modified starch is formed by reacting waxy corn starch with a hydrophilic modifier and then grafting a hydrophobic monomer onto the waxy corn starch through free polymerization. Compared with the prior art, the invention has the following advantages: the amphiphilic starch fluid loss agent has high-temperature resistance and can be used at 130-150 ℃; the amphiphilic starch resists monovalent salt to saturated saline and divalent salt to 5.0 percent; the amphiphilic starch has little influence on the viscosity of the drilling fluid; the amphiphilic starch can be completely biodegraded, has no biotoxicity and has no influence on the environment; the oil-based drilling fluid has certain oil dispersibility and can be used as a fluid loss additive of an oil-based drilling fluid; the compatibility of the amphiphilic starch and various drilling fluid treating agents is good.
Description
Technical Field
The invention relates to a preparation method of an amphiphilic starch filtrate reducer for water-based drilling fluid, which is used in the drilling process of petroleum exploration wells and production wells.
Background
At present, only etherified starch is used as a water-based fluid loss additive in the field of drilling, but the temperature resistance of the etherified starch is only about 100 ℃, the salt resistance is poor, and the etherified starch cannot be used in oil-based drilling fluid, so that the application range of the etherified starch is greatly limited. Other modification approaches, such as grafting, crosslinking and other composite modification, have more research reports, but the product has complex process, more impurities, higher cost, poor environmental protection and very little actual field application. Therefore, the problem that needs to be solved at present is to produce the amphiphilic starch treating agent for the temperature-resistant and salt-resistant drilling fluid by adopting a simple and low-cost synthesis process. At present, only etherified starch is used as a water-based filtrate reducer in the field of drilling, but the temperature resistance of the etherified starch is only about 100 ℃, and in solid-free drilling fluid, when the downhole temperature reaches 100 ℃, the etherified starch needs to be supplemented in large quantity to offset the temperature loss, so that the drilling fluid is frequently regulated and controlled, and the labor capacity, the cost and the drilling risk are increased. And the etherified starch has poor salt resistance and cannot be used in the oil-based drilling fluid, so that the application range of the etherified starch is greatly limited. Other modification approaches, such as grafting, crosslinking and other composite modification, have more research reports, but the product has complex process, more impurities, higher cost, poor environmental protection and very little actual field application. The method for preparing the amphiphilic starch comprises the following step of carrying out hydrophobic modification on corymbose ships, williams, etc. (college chemical engineering journal, 2011, 25(5): 832-charge 837; patent CN 201010133212.9) by using carboxymethyl starch as a raw material and benzoyl chloride, etc. as a hydrophobic reagent for direct grafting, wherein the starch is used as a reservoir protection treating agent in the drilling fluid, and the permeability recovery value is more than 90%. Up to now, there has been no report of the use of amphiphilic starch as a fluid loss additive for water-based drilling fluids. The new synthesis method is adopted, the temperature resistance and salt tolerance of the starch are improved, and the application range is expanded. At present, the development of a synthetic method with simple process and low cost for producing the amphiphilic starch fluid loss additive with temperature resistance and salt resistance is urgently needed. The invention aims to overcome the defects of the prior art and provide the amphiphilic fluid loss additive which has strong temperature resistance and divalent salt resistance and can effectively reduce the fluid loss of water-based drilling fluid. According to the invention, waxy corn starch is firstly reacted with a hydrophilic modifier, and then a hydrophobic monomer is grafted to the waxy corn starch through a free polymerization reaction, so that the formed amphiphilic starch can be used as a fluid loss additive of drilling fluid.
Disclosure of Invention
The invention aims to provide a preparation method of an amphiphilic starch fluid loss additive for water-based drilling fluid, which is formed by reacting waxy corn starch with a hydrophilic modifier and grafting a hydrophobic monomer onto the waxy corn starch through free polymerization.
In a preferred embodiment of the present invention, the amphiphilic starch fluid loss additive for water-based drilling fluids comprises: 1000 parts of starch, 500 parts of sodium hydroxide 200-; the components are all in parts by mass (g).
In a preferred embodiment of the invention, the starch is selected from waxy maize starch having a relative molecular mass of 5.7 to 8.1 ten thousand and an amylopectin content of more than 98%.
In a preferred embodiment of the invention, the methanol may be replaced by equal mass of ethanol, propanol or isopropanol.
In a preferred embodiment of the present invention, the hydrophobic monomer is selected from any one of 3-phenyl-2-acrylic acid, acrylonitrile and acrylic acid.
In a preferred embodiment of the present invention, the initiator is selected from any one of ammonium persulfate, potassium persulfate, dibenzoyl peroxide, cyclohexanone peroxide, and t-butyl hydroperoxide.
According to another aspect of the invention, a preparation method of the amphiphilic starch fluid loss additive for the water-based drilling fluid is provided, and comprises the following steps:
(1) weighing 1000 parts of starch, adding the starch into a three-neck flask, then adding 100-300 parts of methanol, placing the three-neck flask in a water bath with the temperature of 35 ℃, and stirring for 30 minutes;
(2) sequentially adding 100-300 parts of sodium hydroxide and 2000-3000 parts of water, and continuing stirring for 30 minutes;
(3) sequentially adding 100-200 parts of sodium hydroxide, 300-500 parts of chloroacetic acid and 200-300 parts of methanol, heating to 60 ℃, and reacting for 60-80 minutes;
(4) cooling to room temperature, sequentially adding 100 and 200 parts of sodium carbonate and 0.5-1.0 part of chloroform, and continuing stirring for 10 minutes;
(5) sequentially adding 100 plus 200 parts of sodium carbonate and 800 plus 1800 parts of hydrophobic monomer, heating to 40-50 ℃, stirring for 30-40 minutes, and introducing nitrogen during the period;
(6) adding 10-20 parts of initiator, heating to 70-80 ℃, and continuing to react for 120- "180 minutes;
(7) stopping stirring, cooling the temperature to room temperature, continuously standing for 120-180 minutes, and discharging;
(8) centrifugal separation, washing with deionized water for 3 times, filtering with filter paper, washing the filtered product with organic solvent for 3-5 times, drying in vacuum drying oven at 70 deg.C, and pulverizing to obtain the final product.
Preferably, in the preparation method, the stirring speed is 300-500 rpm.
Preferably, in the above preparation method, the room temperature is 10 to 25 ℃, preferably 25 ℃.
Preferably, in the above production method, the reaction temperatures in the steps (5) and (6) are 45 ℃ and 75 ℃, respectively.
Preferably, in the above production method, the reaction times in the steps (3), (5), (6) and (7) are 70 minutes, 35 minutes, 150 minutes and 150 minutes, respectively.
Preferably, in the above preparation method, the number of times of centrifugation in the step (8) is 4.
Preferably, in the above preparation method, the organic solvent is selected from any one of ethanol, propanol, hexane, isopropanol, and petroleum ether.
According to one aspect of the invention, the amphiphilic starch fluid loss additive for the water-based drilling fluid is provided, and has the following structural formula:
compared with the prior art, the invention has the following advantages: the amphiphilic starch fluid loss agent has high-temperature resistance and can be used at 130-150 ℃; the amphiphilic starch resists monovalent salt to saturated saline and divalent salt to 5.0 percent; the amphiphilic starch has little influence on the viscosity of the drilling fluid; the amphiphilic starch can be completely biodegraded, has no biotoxicity and has no influence on the environment; the oil-based drilling fluid has certain oil dispersibility and can be used as a fluid loss additive of an oil-based drilling fluid; the compatibility of the amphiphilic starch and various drilling fluid treating agents is good.
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Detailed Description
The invention is further illustrated with reference to examples.
Example 1:
weighing 1000 parts of starch, adding the starch into a three-neck flask, then adding 100 parts of methanol, placing the three-neck flask in a water bath with the temperature of 35 ℃, and stirring for 30 minutes at the rotating speed of 300 revolutions per minute; sequentially adding 100 parts of sodium hydroxide and 2000 parts of water, and continuously stirring for 30 minutes; sequentially adding 100 parts of sodium hydroxide, 300 parts of chloroacetic acid and 200 parts of methanol, heating to 60 ℃, and reacting for 60 minutes; cooling to room temperature (10 ℃), sequentially adding 100 parts of sodium carbonate and 0.5 part of chloroform, and continuing stirring for 10 minutes; sequentially adding 100 parts of sodium carbonate and 800 parts of acrylic acid, heating to 40 ℃, stirring at the rotating speed of 500 revolutions per minute for 30 minutes, and introducing nitrogen gas during the stirring; adding 10 parts of ammonium persulfate, heating to 70 ℃, and continuing to react for 120 minutes; stopping stirring, cooling to room temperature (10 ℃), standing for 120 minutes, and discharging; and (3) centrifugally separating, washing with deionized water for 3 times, filtering by using filter paper, washing the filtered product with propanol for 3 times, drying in a vacuum drying oven at 70 ℃, and crushing to obtain the product.
Example 2:
weighing 1000 parts of starch, adding the starch into a three-neck flask, then adding 200 parts of methanol, placing the three-neck flask in a water bath with the temperature of 35 ℃, and stirring for 30 minutes at the rotating speed of 300 revolutions per minute; sequentially adding 150 parts of sodium hydroxide and 2500 parts of water, and continuously stirring for 30 minutes; sequentially adding 100 parts of sodium hydroxide, 400 parts of chloroacetic acid and 200 parts of methanol, heating to 60 ℃, and reacting for 70 minutes; cooling to room temperature (15 ℃), sequentially adding 150 parts of sodium carbonate and 1.0 part of chloroform, and continuing stirring for 10 minutes; adding 200 parts of sodium carbonate and 1500 parts of 3-phenyl-2-acrylic acid in sequence, heating to 50 ℃, stirring at the rotating speed of 500 revolutions per minute for 35 minutes, and introducing nitrogen during the stirring; adding 15 parts of potassium persulfate, heating to 75 ℃, and continuing to react for 160 minutes; stopping stirring, cooling to room temperature (15 ℃), standing for 150 minutes, and discharging; centrifugal separation, washing with deionized water for 3 times, filtering with filter paper, washing the filtered product with isopropanol for 5 times, drying in a vacuum drying oven at 70 deg.C, and pulverizing to obtain the final product.
Example 3:
weighing 1000 parts of starch, adding the starch into a three-neck flask, then adding 300 parts of methanol, placing the three-neck flask in a water bath with the temperature of 35 ℃, and stirring for 30 minutes at the rotating speed of 300 revolutions per minute; sequentially adding 200 parts of sodium hydroxide and 3000 parts of water, and continuously stirring for 30 minutes; sequentially adding 200 parts of sodium hydroxide, 500 parts of chloroacetic acid and 300 parts of methanol, heating to 60 ℃, and reacting for 80 minutes; cooling to room temperature (25 ℃), sequentially adding 200 parts of sodium carbonate and 0.8 part of chloroform, and continuing stirring for 10 minutes; sequentially adding 150 parts of sodium carbonate and 1800 parts of acrylonitrile, heating to 40 ℃, stirring at the rotating speed of 500 revolutions per minute for 40 minutes, and introducing nitrogen; adding 20 parts of cyclohexanone peroxide, heating to 80 ℃, and continuing to react for 180 minutes; stopping stirring, cooling to room temperature (25 ℃), standing for 180 minutes, and discharging; centrifugal separation, washing with deionized water for 5 times, filtering with filter paper, washing the filtered product with petroleum ether for 4 times, drying in a vacuum drying oven at 70 deg.C, and pulverizing to obtain the final product.
Evaluation of the products of the examples:
the amphiphilic property of the product is detected by adopting a contact angle method, and the water phase contact angle measurement method comprises the following steps: (1) sieving the pulverized product with 1000 mesh sieve, and subjecting the obtained fine powder to a pressure of 400 kg/cm2(the pressing time is controlled to be 5 minutes), and a relatively smooth disk body (with uniform roughness) with the diameter of 1.0 cm and the thickness of 0.1 cm is prepared for standby; (2) placing the prepared powder tray body in a wide-mouth transparent glass container (with the bottom kept flat) with the inner diameter of 4.0 cm; (3) then slowly pouring a certain volume of paraffin oil; (4) after balancing for 30 minutes, injecting deionized water drops with the volume of 1.0-10 microliters by using a micro injector, enabling the water drops to slowly move in an oil layer and contact with the surface of a disc body, and immediately tracking and recording the shape change of the water drops by using a high-precision CCD camera; (5) intercepting a photo group with relatively stable water drop appearance within a certain time (1-5 seconds), and analyzing and calculating by using appearance analysis software to obtain a contact angle theta; (6) repeating the operation, and taking the average value of the contact angles measured for several times to obtain the water phase contact angle (advancing angle) of the amphiphilic starch.
The method for measuring the oil phase contact angle is similar to that for measuring the water phase contact angle, and is characterized in that the paraffin oil is changed into deionized water in a wide-mouth glass container, a prepared powder disc is gently placed to be just contacted with the liquid surface, the powder disc is suspended, a certain amount of paraffin oil is extracted by a micro-injector and slowly placed at the bottom of the glass container, the injector is pushed to slowly form 1.0-10 microliter of oil drops, then the shape change of the oil drops when the oil drops are contacted with the powder disc after rising to the top is tracked and recorded, and the oil phase contact angle of the amphiphilic starch can be obtained by leveling after multiple measurements. The water phase and oil phase contact angles were measured for example 1, example 2 and example 3, respectively, and the results are shown in table 1.
TABLE 1 contact Angle measurement results
As can be seen from the results in Table 1, the contact angles of water phase were between 35 ° and 56 ° and the contact angles of oil phase were between 39 ° and 54 ° for all three products of example 1, example 2 and example 3, which fully demonstrates the good amphiphilicity of the products of the present invention.
The performance of the amphiphilic starch fluid loss additive is determined based on the basic formula of the water-based drilling fluid commonly used on site. The formula of the No. 1 conventional water-based drilling fluid is as follows: 3.0% of bentonite and 0.5% of Na2CO3+ 0.5% IND30 polymer coating agent +3.0% SD102 carboxymethyl sulfonated phenolic resin +3.0% nanoemulsion + 1.0% aminopolyol + 0.5% aluminum based polymer weighted with barite to a density of 1.10g/cm3(ii) a The 2# saturated saline drilling fluid comprises the following components in percentage by weight: 3.0% of bentonite and 0.5% of Na2CO3+ 5.0% SMP-2 sulfonated phenolic resin + 5.0% SMC sulfonated lignite + 1.0% FCLS iron chromium lignosulfonate + 0.5% CMC-LV low viscosity carboxymethyl cellulose + 0.2% PAC polyanionic cellulose + 0.2% caustic soda + 0.2% AS sodium alkylsulfate + NaCl to saturation, weighted with barite to a density of 1.30g/cm3；3# CaCl2The formula of the brine is as follows: 3.0% of bentonite and 4.0% of CaCl2Calcium chloride + 2.0% NH4HPAN hydrolyzed polyacrylonitrile ammonium salt + 1.0% PAC-LV low-viscosity carboxymethyl cellulose + 0.6% SCM carboxymethyl starch +3.0% QS-2 ultrafine calcium carbonate + 2.0% FT-1 sulfonated asphalt + 0.3% NaOH sodium hydroxide + 0.2% XC xanthan gum + 0.3% KPAM polyacrylamide potassium salt, weighted with barite to a density of 1.20g/cm3。
And 2.0% of amphiphilic starch is added on the basis of the 1#, 2# and 3# slurries respectively, and the influence of the amphiphilic starch on the water-based drilling fluid is examined. The change in properties before and after rolling at 150 ℃ for 16 hours was examined and the results are shown in Table 2.
TABLE 2 Effect of amphiphilic starch on Water-based drilling fluids Performance
The specific test method is described in GB/T16783-1997 water-based drilling fluid field test program, whereinFV is the funnel viscosity of the water-based drilling fluid, PV is the plastic viscosity of the water-based drilling fluid, YP is the yield value of the water-based drilling fluid, the initial and final cut are the shear forces measured after 10 seconds and 10 minutes of rest, APIFLHTHP, which is a water loss at normal temperature and pressureFLThe water is lost at high temperature and high pressure.
As can be seen from the results in Table 1, the amphiphilic starch of the invention has an outstanding fluid loss reducing function in three different water-based drilling fluid systems, the API fluid loss and the high-temperature and high-pressure fluid loss are both greatly reduced, and the plastic viscosity, the shearing force and the initial and final shearing change are not large. Through comparison, the amphiphilic starch disclosed by the invention can resist saturated saline water, resist calcium chloride to 4.0%, resist temperature to 150 ℃, and has a good application prospect.
The biotoxicity of the amphiphilic starch was tested by the luminophore method using a DXY-2 biotoxicity tester according to GB/T15441-1995 "luminophore method for determination of acute toxicity of Water quality". The detection results of example 1, example 2 and example 3 are respectively: LC (liquid Crystal)50Values of 650,000, 587,000 and 625,000, respectively, far exceeding the non-toxic standard: (>30,000), which is a good indication of the environmental friendliness of such treatments.
Claims (7)
1. A preparation method of an amphiphilic starch fluid loss additive for water-based drilling fluid is characterized by comprising the following steps:
(1) weighing 1000 parts of starch, adding the starch into a three-neck flask, then adding 100-300 parts of methanol, placing the three-neck flask in a water bath with the temperature of 35 ℃, and stirring for 30 minutes;
(2) sequentially adding 100-300 parts of sodium hydroxide and 2000-3000 parts of water, and continuing stirring for 30 minutes;
(3) sequentially adding 100-200 parts of sodium hydroxide, 300-500 parts of chloroacetic acid and 200-300 parts of methanol, heating to 60 ℃, and reacting for 60-80 minutes;
(4) cooling to room temperature, sequentially adding 100 and 200 parts of sodium carbonate and 0.5-1.0 part of chloroform, and continuing stirring for 10 minutes;
(5) sequentially adding 100-200 parts of sodium carbonate and 800-1800 parts of 3-phenyl-2-acrylic acid or acrylonitrile or acrylic acid, heating to 40-50 ℃, stirring for 30-40 minutes, and introducing nitrogen during the stirring;
(6) adding 10-20 parts of initiator, heating to 70-80 ℃, and continuing to react for 120- "180 minutes;
(7) stopping stirring, cooling the temperature to room temperature, continuously standing for 120-180 minutes, and discharging;
(8) centrifuging, washing with deionized water for 3 times, filtering with filter paper, washing the filtered product with organic solvent for 3-5 times, drying in a vacuum drying oven at 70 deg.C, and pulverizing to obtain the final product; the stirring speed is 300-500 rpm; the room temperature is 10-25 ℃; the reaction temperatures in the steps (5) and (6) are 45 ℃ and 75 ℃ respectively.
2. The preparation method of the amphiphilic starch fluid loss additive for the water-based drilling fluid according to claim 1, wherein the organic solvent is selected from any one of ethanol, propanol, hexane, isopropanol and petroleum ether
3. The method for preparing the amphiphilic starch fluid loss additive for the water-based drilling fluid according to claim 1, wherein the starch is selected from waxy corn starch, the relative molecular mass of the waxy corn starch is 5.7-8.1 ten thousand, and the amylopectin content of the waxy corn starch is more than 98%.
4. The method for preparing the amphiphilic starch fluid loss additive for the water-based drilling fluid according to claim 1, wherein the methanol can be replaced by ethanol, propanol or isopropanol with equal mass.
5. The preparation method of the amphiphilic starch fluid loss additive for the water-based drilling fluid according to claim 1, wherein the initiator is selected from any one of ammonium persulfate, potassium persulfate, dibenzoyl peroxide, cyclohexanone peroxide and tert-butyl hydroperoxide.
6. The preparation method of the amphiphilic starch fluid loss additive for the water-based drilling fluid according to any one of claims 1 to 5, wherein the reaction time in the steps (3), (5), (6) and (7) is 70 minutes, 35 minutes, 150 minutes and 150 minutes respectively.
7. The method for preparing the amphiphilic starch fluid loss additive for the water-based drilling fluid according to any one of claims 1 to 5, wherein the centrifugation in the step (8) is performed for 4 times.
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| WO2016167751A1 (en) * | 2015-04-14 | 2016-10-20 | Halliburton Energy Services, Inc. | Methods of cleaning invert emulsion drilling fluids |
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| US20060052577A1 (en) * | 2001-02-06 | 2006-03-09 | Graham Swift | Methods of synthesis of polymers and copolymers from natural products |
| CN101787267B (en) * | 2010-03-17 | 2012-10-17 | 西南石油大学 | Double-modified starch fluid loss additive used for oil and gas field drilling fluid and preparation method thereof |
| CN102898585B (en) * | 2011-07-26 | 2015-05-13 | 四川仁智油田技术服务股份有限公司 | Preparation method of high temperature resistant drilling fluid filtrate reducer |
| CN102585784B (en) * | 2011-12-30 | 2013-11-20 | 中国石油集团川庆钻探工程有限公司 | Filtrate reducer for water-based drilling fluid and preparation method of filtrate reducer |
| US20140186626A1 (en) * | 2012-09-19 | 2014-07-03 | Sinopec Research Institute Of Petroleum Engineering | Modified starch, preparation method and use of the same, and drilling fluid |
| CN105778872A (en) * | 2014-12-22 | 2016-07-20 | 中石化胜利石油工程有限公司钻井工艺研究院 | Amphiphilic starch filtrate loss reducer for water base drilling fluid and preparation method thereof |
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| Graft copolymerization of acrylamide onto carboxymethyl starch;Cao, YM; Qing, XS; Sun, J; 等.;《EUROPEAN POLYMER JOURNAL》;20020930;第38卷(第9期);第1921-1924页 * |
| 国内水基钻井液降滤失剂研究现状;李财富; 李本高; 汪燮卿;《中外能源》;20130215(第2期);第39-44页 * |
| 淀粉改性研究及其在钻井液中的应用;孔勇; 杨枝; 王治法; 杨小华;《应用化工》;20161018(第11期);第2153-2157页 * |
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Effective date of registration: 20210914 Address after: 100027 Chaoyangmen North Street, Chaoyang District, Chaoyang District, Beijing Patentee after: SINOPEC Group Patentee after: SINOPEC OILFIELD SERVICE Corp. Patentee after: SINOPEC SHENGLI PETROLEUM ENGINEERING Co.,Ltd. Patentee after: SINOPEC SHENGLI PETROLEUM ENGINEERING CO., LTD. DRILLING TECHNOLOGY Research Institute Address before: 100101 Beichen West Road, Chaoyang District, Beijing 8 Beichen world center, block A 703. Patentee before: SINOPEC OILFIELD SERVICE Corp. Patentee before: SINOPEC SHENGLI PETROLEUM ENGINEERING Co.,Ltd. Patentee before: SINOPEC SHENGLI PETROLEUM ENGINEERING CO., LTD. DRILLING TECHNOLOGY Research Institute |
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| TR01 | Transfer of patent right |
Effective date of registration: 20220908 Address after: No. 22, Chaoyangmen North Street, Chaoyang District, Beijing 100725 Patentee after: SINOPEC Group Patentee after: SINOPEC OILFIELD SERVICE Corp. Patentee after: SINOPEC SHENGLI PETROLEUM ENGINEERING Co.,Ltd. Patentee after: Drilling fluid technology service center of Sinopec Shengli Petroleum Engineering Co.,Ltd. Address before: 100027 Chaoyangmen North Street, Chaoyang District, Chaoyang District, Beijing Patentee before: SINOPEC Group Patentee before: SINOPEC OILFIELD SERVICE Corp. Patentee before: SINOPEC SHENGLI PETROLEUM ENGINEERING Co.,Ltd. Patentee before: SINOPEC SHENGLI PETROLEUM ENGINEERING CO., LTD. DRILLING TECHNOLOGY Research Institute |